CN105702388A - Heat processing method of Bi-2212 superconducting wire/strip material - Google Patents
Heat processing method of Bi-2212 superconducting wire/strip material Download PDFInfo
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a heat processing method of a Bi-2212 superconducting wire/strip material. The method comprises following steps of firstly, placing a Bi-2212 multi-core wire/strip material in a processing furnace; importing oxygen and nitrogen mixed gas or oxygen and argon mixed gas in the processing furnace so as to remove air in the furnace; secondly, continuing to import oxygen and nitrogen mixed gas or oxygen and argon mixed gas; under a condition of constant furnace pressure and oxygen partial pressure, carrying out partial melting heat processing to the Bi-2212 multi-core wire/strip material; and thirdly, stopping importing the oxygen and nitrogen mixed gas or oxygen and argon mixed gas, after removing the gas, obtaining the Bi-2212 superconducting wire/strip material. According to the method provided by the invention, the gas expansion in the Bi-2212 multi-core wire/strip material can be effectively inhibited; the bubbling or defect resulting from the bubbling can be prevented; moreover, the density of the core thread can be improved; and the even Bi-2212 superconducting wire/strip material with high performance can be obtained.
Description
Technical field
The invention belongs to high temperature superconducting materia preparing technical field, be specifically related to the heat treatment method of a kind of Bi-2212 superconducting wires/strips。
Background technology
Due to Bi2Sr2CaCu2Ox(Bi-2212) wire rod high-temperature superconductor has the low temperature highfield current-carrying performance of excellence, and be the currently the only practical-HTS materials preparing into isotropism round wires, above-mentioned characteristic makes Bi-2212 high-temperature superconductor material become the preferred material preparing low temperature high field magnet inside coil。
The technology of preparing that current powder-in-tube technique (PIT) and fusion method combine is to prepare high-performance
The mainstream technology of Bi-2212 wire rod。This technology is that superconducting precursor powder end loads silver pipe, prepares into multicore complex by drawing, assembling, and reprocessing, to the wire size of design, then carries out part fusing heat treatment and can obtain the Bi-2212 superconducting wire of superior performance。
Powder-in-tube technique, is encased in metal tube by powder and makes complex, after complex is processed。But powder loads in silver pipe process, and the gas of powder surface absorption and powder gap gas are together loaded in silver pipe, and after drawing is processed, majority of gas is sealed in final wire rod。At the heating initial stage, the gas being sealed in wire rod expands according to gay lussacs law, and under the constraint of jacket, gas volume remains unchanged。When being warming up to core filaments fusion temperature, the gases at high pressure being sealed in Bi-2212 wire internal occupy certain volume, the existence of gases at high pressure makes part Bi-2212 molten mass be arranged, and owing to Bi-2212 wire core filament diameter only has 20 μm, the Bi-2212 molten mass of some position assembling more gas core filaments is arranged completely, causes that this section of core filaments quenches completely；The Bi-2212 core filaments assembling not many gas forms the pore space structure of spongy body shape, causes being formed between most of superconduction crystal grain big mispairing angle, has had a strong impact on the supercurrent circulation at intergranular, significantly reduced the critical current of Bi-2212 wire rod。On the other hand, in temperature-rise period, wire rod ambient outside air pressure remains unchanged, increase with temperature, wire rod inside and outside differential pressure is gradually increased, temperature reaches to a certain degree, the internal pressure produced of core filaments and the ambient atmos pressure difference of assembling a large amount of gas exceed the limit that sheath material deforms, jacket will expand, cause that bag sleeving inner space increases, continue to be warmed up to core filaments fusion temperature, there will be the less cavernous structure of Bi-2212 density that more serious core filaments is arranged completely or formed, cause that wire rod current-carrying performance is lower, and the expanded creep limit exceeding greatly sheath material of wire rod core filaments that excessively serious air accumulation causes, cause wire rod core filaments that pore even crackle occurs, there is serious seepage in what cause wire rod, leverage the use of wire rod。
Summary of the invention
The technical problem to be solved is in that for above-mentioned the deficiencies in the prior art, it is provided that the heat treatment method of a kind of Bi-2212 superconducting wires/strips。The method can effectively suppress the expansion of wire internal gas, effectively prevent bubbling or defect that bubbling brings, can improve core filaments density simultaneously, it is possible to obtains that performance is high and uniform Bi-2212 superconducting wires/strips。
For solving above-mentioned technical problem, the technical solution used in the present invention is: the heat treatment method of a kind of Bi-2212 superconducting wires/strips, it is characterised in that the method comprises the following steps:
Step one, Bi-2212 multicore wire/belt material is placed in heat-treatment furnace, then passes into oxygen-nitrogen mixture body or oxygen argon mixture gas in heat treated stove to get rid of furnace air；
Step 2, get rid of in step one in the heat-treatment furnace of air and continued to pass into oxygen-nitrogen mixture body or oxygen argon mixture gas, constant in 20atm～200atm at furnace pressure, partial pressure of oxygen constant for 0.5atm～1atm when, 20min～30min it is incubated after Bi-2212 multicore wire/belt material is first warming up to 880 DEG C～900 DEG C, then it is incubated 24h～48h after being cooled to 810 DEG C～850 DEG C, cools to 25 DEG C of room temperatures afterwards with the furnace；
Step 3, stop in step 2 cooling after heat-treatment furnace in pass into oxygen-nitrogen mixture body or oxygen argon mixture gas, then the oxygen-nitrogen mixture body in heat-treatment furnace or oxygen argon mixture gas are discharged until furnace pressure reduces to normal pressure, obtain Bi-2212 superconducting wires/strips。
The heat treatment method of above-mentioned a kind of Bi-2212 superconducting wires/strips, it is characterised in that the core number of the wire/belt material of Bi-2212 multicore described in step one is 49～7725 cores。
The heat treatment method of above-mentioned a kind of Bi-2212 superconducting wires/strips, it is characterised in that the speed heated up described in step 2 is 50 DEG C/h～100 DEG C/h。
The heat treatment method of above-mentioned a kind of Bi-2212 superconducting wires/strips, it is characterised in that described in step 2, the speed of cooling is 1 DEG C/h～10 DEG C/h。
The heat treatment method of above-mentioned a kind of Bi-2212 superconducting wires/strips, it is characterised in that oxygen-nitrogen mixture body or the rate of discharge of oxygen argon mixture gas in heat-treatment furnace described in step 3 are make the pressure in heat-treatment furnace with the rate reduction of 2MPa/h～5MPa/h。
The present invention compared with prior art has the advantage that
1, preparation technology of the present invention is simple, reasonable in design, low cost of manufacture, and face of promoting is big, is beneficial to the production being applied to the long line of Bi-2212。
2, the heat treatment method of Bi-2212 superconducting wires/strips of the present invention can effectively prevent Bi-2212 wire/belt material core filaments from hole or bubbling occur。
3, Bi-2212 multicore wire/belt material pressure of external environment in heat treatment process of the present invention is bigger, effectively inhibit the expansion of internal gas, effectively prevent bubbling or defect that bubbling brings, core filaments density can be improved simultaneously, finally give that performance is high and uniform Bi-2212 superconducting wires/strips。
4, the core filaments density of Bi-2212 superconducting wires/strips prepared after heat treatment of the present invention nearly reaches solid density (the core filaments density of conventional wire/belt material is only about 65%), and its engineering critical current density reaches 400～500A/mm2(4.2K, 20T), is about 1.3～1.5 times of conventional line/material current-carrying performance, and bubbling do not occur in wire/belt material, ooze the defect such as a little, and the uniformity of wire/belt material current-carrying performance is within ± 5%。
Below in conjunction with embodiment, the present invention is described in further detail。
Detailed description of the invention
Embodiment 1
The heat treatment method of the present embodiment Bi-2212 superconducting wire comprises the following steps:
Step one, being 2mm by diameter, the Bi-2212 Multi-core wire that core number is 666 cores is placed in heat-treatment furnace, then passes into oxygen argon mixture gas that oxygen volume content is 1% in heat treated stove to get rid of furnace air；
Step 2, get rid of in step one in the heat-treatment furnace of air and continued to pass into the oxygen argon mixture gas that oxygen volume content is 1%, constant in 100atm at furnace pressure, partial pressure of oxygen constant for 1atm when, insulation 25min after Bi-2212 Multi-core wire is first warming up to 890 DEG C with the heating rate of 80 DEG C/h, then it is incubated 30h after being cooled to 830 DEG C with the rate of temperature fall of 8 DEG C/h, cools to 25 DEG C of room temperatures afterwards with the furnace；
Step 3, stop in step 2 cooling after heat-treatment furnace in pass into the oxygen argon mixture gas that oxygen volume content is 1%, then the oxygen argon mixture gas in heat-treatment furnace is discharged until furnace pressure reduces to normal pressure (normal pressure refers to an atmospheric pressure), obtain Bi-2212 superconducting wire；The rate of discharge of the oxygen argon mixture gas in described heat-treatment furnace is make the pressure in heat-treatment furnace with the rate reduction of 3MPa/h。
The core filaments density of Bi-2212 multi-core superconducting wire rod prepared after the present embodiment heat treatment reaches solid density more than 99% (the core filaments density of conventional strand is only about 65%), and its engineering critical current density reaches 450A/mm2(4.2K, 20T), is about 1.5 times of conventional strand current-carrying performance, and bubbling do not occur in wire rod, ooze the defect such as a little, and the uniformity of wire rod current-carrying performance is within ± 5%。
Embodiment 2
The heat treatment method of the present embodiment Bi-2212 superconducting tape comprises the following steps:
Step one, being 1.5mm by thickness, the Bi-2212 multi-filamentary tape that core number is 595 cores is placed in heat-treatment furnace, then passes into oxygen-nitrogen mixture body that oxygen volume content is 1% in heat treated stove to get rid of furnace air；
Step 2, get rid of in step one in the heat-treatment furnace of air and continued to pass into the oxygen-nitrogen mixture body that oxygen volume content is 1%, constant in 50atm at furnace pressure, partial pressure of oxygen constant for 0.5atm when, insulation 25min after Bi-2212 multi-filamentary tape is first warming up to 880 DEG C with the heating rate of 60 DEG C/h, then it is incubated 40h after being cooled to 830 DEG C with the rate of temperature fall of 5 DEG C/h, cools to 25 DEG C of room temperatures afterwards with the furnace；
Step 3, stop in step 2 cooling after heat-treatment furnace in pass into the oxygen-nitrogen mixture body that oxygen volume content is 1%, oxygen-nitrogen mixture body in heat-treatment furnace is discharged until furnace pressure reduces to normal pressure (normal pressure refers to an atmospheric pressure), obtains Bi-2212 superconducting tape；The rate of discharge of the oxygen-nitrogen mixture body in described heat-treatment furnace is make the pressure in heat-treatment furnace with the rate reduction of 3MPa/h。
The core filaments density of Bi-2212 superconducting tape prepared after the present embodiment heat treatment reaches solid density more than 90% (the core filaments density of conventional band is only about 65%), and its engineering critical current density reaches 400A/mm2(4.2K, 20T), is about 1.33 times of conventional band current-carrying performance, and bubbling do not occur in band, ooze the defect such as a little, and the uniformity of current-carrying performance is within ± 5%。
Embodiment 3
The heat treatment method of the present embodiment Bi-2212 superconducting wire comprises the following steps:
Step one, being 1mm by diameter, the Bi-2212 Multi-core wire that core number is 1530 cores is placed in heat-treatment furnace, then passes into oxygen-nitrogen mixture body that oxygen volume content is 0.5% in heat treated stove to get rid of furnace air；
Step 2, get rid of in step one in the heat-treatment furnace of air and continued to pass into the oxygen-nitrogen mixture body that oxygen volume content is 0.5%, constant in 200atm at furnace pressure, partial pressure of oxygen constant for 1atm when, insulation 30min after Bi-2212 Multi-core wire is first warming up to 880 DEG C with the heating rate of 80 DEG C/h, then it is incubated 40h after being cooled to 830 DEG C with the rate of temperature fall of 10 DEG C/h, cools to 25 DEG C of room temperatures afterwards with the furnace；
Step 3, stop in step 2 cooling after heat-treatment furnace in pass into the oxygen-nitrogen mixture body that oxygen volume content is 0.5%, oxygen-nitrogen mixture body in heat-treatment furnace is discharged until furnace pressure reduces to normal pressure (normal pressure refers to an atmospheric pressure), obtains Bi-2212 superconducting wire；The rate of discharge of the oxygen-nitrogen mixture body in described heat-treatment furnace is make the pressure in heat-treatment furnace with the rate reduction of 2MPa/h。
The core filaments density of Bi-2212 superconducting wire prepared after the present embodiment heat treatment nearly reaches solid density (the core filaments density of conventional strand is only about 65%), and its engineering critical current density reaches 500A/mm2(4.2K, 20T), is about 1.67 times of conventional strand current-carrying performance, and bubbling do not occur in wire rod, ooze the defect such as a little, and the uniformity of wire rod current-carrying performance is within ± 5%。
Embodiment 4
The heat treatment method of the present embodiment Bi-2212 superconducting tape comprises the following steps:
Step one, being 2.5mm by thickness, the Bi-2212 multi-filamentary tape that core number is 7725 cores is placed in heat-treatment furnace, then passes into oxygen argon mixture gas that oxygen volume content is 0.3% in heat treated stove to get rid of furnace air；
Step 2, get rid of in step one in the heat-treatment furnace of air and continued to pass into the oxygen argon mixture gas that oxygen volume content is 0.3%, constant in 200atm at furnace pressure, partial pressure of oxygen constant for 0.6atm when, insulation 20min after Bi-2212 multi-filamentary tape is first warming up to 900 DEG C with the heating rate of 70 DEG C/h, then it is incubated 24h after being cooled to 810 DEG C with the rate of temperature fall of 1 DEG C/h, cools to 25 DEG C of room temperatures afterwards with the furnace；
Step 3, stop in step 2 cooling after heat-treatment furnace in pass into the oxygen argon mixture gas that oxygen volume content is 0.3%, oxygen argon mixture gas in heat-treatment furnace is discharged until furnace pressure reduces to normal pressure (normal pressure refers to an atmospheric pressure), obtains Bi-2212 superconducting tape；The rate of discharge of the oxygen argon mixture gas in described heat-treatment furnace is make the pressure in heat-treatment furnace with the rate reduction of 3MPa/h。
The core filaments density of Bi-2212 superconducting tape prepared after the present embodiment heat treatment nearly reaches solid density (the core filaments density of conventional band is only about 65%), and its engineering critical current density reaches 440A/mm2(4.2K, 20T), is about 1.46 times of conventional band current-carrying performance, and bubbling do not occur in band, ooze the defect such as a little, and the uniformity of current-carrying performance is within ± 5%。
Embodiment 5
The heat treatment method of the present embodiment Bi-2212 superconducting wire comprises the following steps:
Step one, being 1.5mm by diameter, the Bi-2212 Multi-core wire that core number is 49 cores is placed in heat-treatment furnace, then passes into oxygen argon mixture gas that oxygen volume content is 2.5% in heat treated stove to get rid of furnace air；
Step 2, get rid of in step one in the heat-treatment furnace of air and continued to pass into the oxygen argon mixture gas that oxygen volume content is 2.5%, constant in 20atm at furnace pressure, partial pressure of oxygen constant for 0.5atm when, insulation 30min after Bi-2212 Multi-core wire is first warming up to 880 DEG C with the heating rate of 50 DEG C/h, then it is incubated 48h after being cooled to 850 DEG C with the rate of temperature fall of 10 DEG C/h, cools to 25 DEG C of room temperatures afterwards with the furnace；
Step 3, stop in step 2 cooling after heat-treatment furnace in pass into the oxygen argon mixture gas that oxygen volume content is 2.5%, oxygen argon mixture gas in heat-treatment furnace is discharged until furnace pressure reduces to normal pressure (normal pressure refers to an atmospheric pressure), obtains Bi-2212 single-core superconducting wire/band or Bi-2212 superconducting wire；The rate of discharge of the oxygen argon mixture gas in described heat-treatment furnace is make the pressure in heat-treatment furnace with the rate reduction of 2MPa/h。
The core filaments density of Bi-2212 superconducting wire prepared after the present embodiment heat treatment nearly reaches solid density (the core filaments density of conventional strand is only about 65%), and its engineering critical current density reaches 460A/mm2(4.2K, 20T), is about 1.53 times of conventional strand current-carrying performance, and bubbling do not occur in wire rod, ooze the defect such as a little, and the uniformity of wire rod current-carrying performance is within ± 5%。
Embodiment 6
The heat treatment method of the present embodiment Bi-2212 superconducting tape comprises the following steps:
Step one, being 2.2mm by thickness, the Bi-2212 multi-filamentary tape that core number is 1530 cores is placed in heat-treatment furnace, then passes into oxygen-nitrogen mixture body that oxygen volume content is 0.5% in heat treated stove to get rid of furnace air；
Step 2, get rid of in step one in the heat-treatment furnace of air and continued to pass into the oxygen-nitrogen mixture body that oxygen volume content is 0.5%, constant in 200atm at furnace pressure, partial pressure of oxygen constant for 1atm when, insulation 30min after Bi-2212 multi-filamentary tape is first warming up to 900 DEG C with the heating rate of 100 DEG C/h, then it is incubated 48h after being cooled to 850 DEG C with the rate of temperature fall of 10 DEG C/h, cools to 25 DEG C of room temperatures afterwards with the furnace；
Step 3, stop in step 2 cooling after heat-treatment furnace in pass into oxygen-nitrogen mixture body or oxygen argon mixture gas, oxygen-nitrogen mixture body in heat-treatment furnace is discharged until furnace pressure reduces to normal pressure (normal pressure refers to an atmospheric pressure), obtains Bi-2212 superconducting tape；The rate of discharge of the oxygen-nitrogen mixture body in described heat-treatment furnace is make the pressure in heat-treatment furnace with the rate reduction of 5MPa/h。
The core filaments density of Bi-2212 superconducting tape prepared after the present embodiment heat treatment nearly reaches solid density (the core filaments density of conventional band is only about 65%), and its engineering critical current density reaches 440A/mm2(4.2K, 20T), is about 1.46 times of conventional band current-carrying performance, and bubbling do not occur in band, ooze the defect such as a little, and the uniformity of band current-carrying performance is within ± 5%。
The above, be only presently preferred embodiments of the present invention, not the present invention is imposed any restrictions。Every any simple modification, change and equivalence change above example made according to inventive technique essence, all still falls within the protection domain of technical solution of the present invention。
Claims (5)
1. the heat treatment method of a Bi-2212 superconducting wires/strips, it is characterised in that the method comprises the following steps:
Step one, Bi-2212 multicore wire/belt material is placed in heat-treatment furnace, then passes into oxygen-nitrogen mixture body or oxygen argon mixture gas in heat treated stove to get rid of furnace air；
Step 2, get rid of in step one in the heat-treatment furnace of air and continued to pass into oxygen-nitrogen mixture body or oxygen argon mixture gas, constant in 20atm～200atm at furnace pressure, partial pressure of oxygen constant for 0.5atm～1atm when, 20min～30min it is incubated after Bi-2212 multicore wire/belt material is first warming up to 880 DEG C～900 DEG C, then it is incubated 24h～48h after being cooled to 810 DEG C～850 DEG C, cools to 25 DEG C of room temperatures afterwards with the furnace；
Step 3, stop in step 2 cooling after heat-treatment furnace in pass into oxygen-nitrogen mixture body or oxygen argon mixture gas, then the oxygen-nitrogen mixture body in heat-treatment furnace or oxygen argon mixture gas are discharged until furnace pressure reduces to normal pressure, obtain Bi-2212 superconducting wires/strips。
2. the heat treatment method of a kind of Bi-2212 superconducting wires/strips according to claim 1, it is characterised in that the core number of the wire/belt material of Bi-2212 multicore described in step one is 49 core～7725 cores。
3. the heat treatment method of a kind of Bi-2212 superconducting wires/strips according to claim 1, it is characterised in that the speed heated up described in step 2 is 50 DEG C/h～100 DEG C/h。
4. the heat treatment method of a kind of Bi-2212 superconducting wires/strips according to claim 1, it is characterised in that described in step 2, the speed of cooling is 1 DEG C/h～10 DEG C/h。
5. the heat treatment method of a kind of Bi-2212 superconducting wires/strips according to claim 1, it is characterized in that, oxygen-nitrogen mixture body or the rate of discharge of oxygen argon mixture gas in heat-treatment furnace described in step 3 are make the pressure in heat-treatment furnace with the rate reduction of 2MPa/h～5MPa/h。
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| CN109524174A (en) * | 2018-11-22 | 2019-03-26 | 西北有色金属研究院 | A kind of preparation method of Bi-2212 hts tape |
| CN109903927A (en) * | 2019-01-30 | 2019-06-18 | 中国科学院电工研究所 | A kind of preparation method of the iron-based superconducting line strips of compound jacket |
| CN110790309A (en) * | 2019-10-30 | 2020-02-14 | 西北有色金属研究院 | Preparation method of Bi-2212 superconducting wire strip |
| CN115287444A (en) * | 2022-09-08 | 2022-11-04 | 西部超导材料科技股份有限公司 | Heat treatment method of Bi-2212 superconducting wire |
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| CN109524174A (en) * | 2018-11-22 | 2019-03-26 | 西北有色金属研究院 | A kind of preparation method of Bi-2212 hts tape |
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